Explosive compound, process of making same and a composition thereof



Patented May 17, 1955 EXPLOSIVE COMPOUND, PROCESS OF MAKING enedinitramine has dissolved to form a water soluble sodium salt. The resulting sodium salt is then converted to the lead salt of ethylenedinitramine by adding to the solution about 66 parts lead nitrate dissolved in about 400 SAME AND A COMPOSITION THEREOF 5 parts water at room temperature. The lead salt is insoluble in the solution and is rapidly formed but agigf g' f f ifi ggg fii g i gg gg fi tation is continued for a few minutes to insure complete Virginia mlXmg of the IWOSPIUUOITS. The suspension 15 then filtered and the precipitate air dried at room temperature N0 Dlawillglfp December 1951, for about sixteen hours. The lead ethylenedinitramine Serial 254,270 can then be loaded without further treatment or purification into oil well gun perforator devices for use at tem- 7 clmms' (CL 52-4) peratures as high as 300 C. or thereabouts.

The foregoing process can be modified in many respects This invention relates to a new compound suitable for without deleteriously aifecting the product. For instance, use as an explosive and to the manufacture thereof. other lead compounds such as lead acetate can be sub- There has been a pressing need in the oil industry for stituted for the lead nitrate and potassium hydroxide can explosives of relatively high heat stability for the purpose be substituted for the sodium hydroxide, if desired. The of firing missiles through the side walls of Well casings far method of mixing the various solutions together can be beneath the earths surface. Numerous types of devices reversed, the reactions can be carried out at elevated have been developed for this purpose, generally known temperatures and drying can be accomplished at elevated as oil Well gun perforators. Gun powder has been used temperatures below that at which the compound would in such devices but has the limitation of being relatively explode. heat sensitive so that upon being lowered to great depths This new explosive due to its low impact and friction premature firing and the like has occurred. The temsensitivity can be handled in the dry state with a reasonperature in such casings, of course, increases with depth able degree of safety while loading, has moderate power of penetration into the earth and for very deep wells or brisance (crushes about 17 grams of sand when initiexplosives of greater heat stability are required. ated in a sand bomb), produces large volumes of gas It is therefore an object of this invention to provide an rather slowly which along with a relatively high flash explosive suitable for use under such higher temperature point are requirements for explosives used in oil well conditions. Another object is to provide a novel properforator guns. Explosive charges consisting of the pellant. Another object of this invention is to provide a lead salt of ethylenedinitramine or in combination with novel compound having characteristics making it emiother heat stable propellants are suitable for operations nently suitable for an explosive. A still further object of of this type. the invention is to provide a novel explosive and a method In addition to having advantages as a propellant, the for the manufacturing thereof. A more specific object compound is useful in ammunition. The ballistic propis to provide improved ammunition priming compositions erties of ammunition and particularly improved ignition as Well as other novel explosive compositions. of the propellant by the primer is obtained with priming The foregoing objects as Well as others which will mixes which contain the lead salt of ethylenedinitramine. become apparent from the following description are While its relatively low impact sensitivity eliminates it as accomplished in accordance with this invention, generally a substitute for the more impact sensitivity normal lead speaking, by providing as the new compound, the lead salt styphnate, mercury fulminate, diazodinitrophenol and of ethylenedinitramine, also referred to herein as lead similar explosives utilized in percussion primers, it can be ethylenedinitramine. The lead salt of ethylenedinitraused in combination with such explosives. Because of mine has been found to be resistant to higher temperaits low impact sensitivity, a priming mix can contain tures than smokeless powder, black powder, nitro-starch, relatively large percentages thereof as an explosive fuel or trinitrotoluene, tetryl, ethylenedinitramine and the like. sensitizer which when ignited by the more impact sensi- Some of such explosives are unsuitable at the higher tive explosive will produce a hot flame, thus improving temperatures because of their relatively low melting the ignition characteristics of the primer and improving points, others because of their relatively low flash points. 5) the ballistics of the cartridge by reducing the number of Hale in U. S. 2,011,578 discloses that ethylenedinitramine squibs, hangfires and other malfunctions due to poor may be used as a substitute for tetryl, picric acid, and triignition. As as example, a priming mix having the folnitrotoluene in booster and high explosive charges but lowing formula has been found to satisfactorily ignite that it explodes spontaneously when heated to 180 C. some of the most difiicultly ignitable propellent powders: In contrast it has been found in accordance with this Pa rts invention that the lead salt or ethylenedimtramine does Diazodinitrophenol 20 not spontaneously explode until temperatures of around Tetracene 5 and abqve e attained a that i is a relatively Lead eth ienediilitlifliilliIIIIIIIIIIIIIIIIII 25 powerful explosive without admlxture with other explo- Calcium silicide 2O sives. It has been found that due to the characteristics Barium nitrate 24 of the lead salt of ethylenedinitrarnine it can be used to Lead peroxide 6 advantage in compositions containing other explosives, as Gum arabic 05 will become apparent hereinafter. 1

In accordance with this invention the lead salt of varfifltlolls can e 111 r going priming comethylenedinitramine is prpared by fi t f i a Soluble pos1tion 111 order to adgust its characteristics for proper alkali metal salt of ethylenedinitramine and then replacing functioning with VariQuS types of p p 1 6X- the alkali metal with lead to effect a precipitation of the p other oxidizers Such as lead nitrate, Potassium insoluble lead salt. As an example of one embodiment nitrate and the like are suitable. Non-explosive fuels of this invention, about 15 parts ethylenedinitramine are other than calcium silicide such as antimony sulfide or a suspended in about 500 parts water at ambient temperametal, for example, zirconium, aluminum and the like,

ture and containing about 16.5 parts sodium hydroxide. The slurry is agitated until substantially all of the ethylmight be advantageous in some priming mixes. Normal lead styphnate and mercury fulminate are examples of other primary explosives which might be substituted for the diazodinitrophenol and in some instances the explosive sensitizer such as tetracene can be eliminated from the composition.

It should be apparent from the foregoing description that the present invention accomplishes its objects and provides a process for making a novel explosive compound and new explosive compositions having unusual characteristics which are advantageous in several types of operations requiring explosive charges.

While specific embodiments have been given and the invention has been described with particularity in the foregoing, modifications which will occur to those skilled in the'art may be made without departing from the spirit and scope of the invention.

Having thus described the invention what is'claimed and desired to secure by Letters Patent is:

1. Lead ethylenedinitramine.

2. A process for making lead ethylenedinitramine which comprises the steps of reacting in solution and in molecular proportions, ethylenedinitramine and an alkali metal hydroxide, reacting, in solution and in molecular proportions, the resulting alkali metal salt of ethylenedinitramine and a lead salt, and thereafter separating the resulting precipitate of lead ethylenedinitramine from the reaction liquor.

3. The process of claim 2 wherein said alkali metal hydroxide is sodium hydroxide.

4. The process of claim 2 wherein said lead salt is water soluble.

Parts Diazodinitrophenol 20 Tetracene 5 Lead ethylenedinitrarnine 25 Calcium silicide 20 Barium nitrate 24 Lead peroxide 6 Gum arabic 0.5

References Cited in the file of this patent UNITED STATES PATENTS Hale Aug. 20, 1935 Herz Jan. 5, 1937 Ashley July 29, 1941 OTHER REFERENCES des Pays Bas, vol. 7, 1888.

Franchimont et al., Recueil des Travoux Chimiques 

1. LEAD ETHYLENEDINITRAMINE.
 2. A PROCESS FOR MAKING LEAD ETHYLENEDINITRAMINE WHICH COMPRISES THE STEPS OF REACTING IN SOLUTION AND IN MOLECULAR PROPORTIONS, ETHYLENEDINITRAMINE AND AN ALKALI METAL HYDROXIDE, REACTING, IN SOLUTION AND IN MOLECULAR PROPORTIONS, THE RESULTING ALKALI METAL SALT OF ETHYLENEDINITRAMINE AND A LEAD SALT, AND THEREAFTER SEPARATING THE RESULTING PRECIPITATE OF LEAD ETHYLENEDINITRAMINE FROM THE REACTION LIQUOR
 7. A PRIMING MIX HAVING A COMPOSITION SUBSTANTIALLY AS FOLLOWS: 